CN112230520A - Water-based PI film stripping liquid and PI film glass method thereof - Google Patents
Water-based PI film stripping liquid and PI film glass method thereof Download PDFInfo
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- CN112230520A CN112230520A CN202011334406.5A CN202011334406A CN112230520A CN 112230520 A CN112230520 A CN 112230520A CN 202011334406 A CN202011334406 A CN 202011334406A CN 112230520 A CN112230520 A CN 112230520A
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
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Abstract
The invention relates to the technical field of stripping liquid, and particularly discloses PI film stripping liquid which comprises the following raw materials in parts by weight: 12-35 parts of water-soluble organic solvent, 3-15 parts of organic amine, 2-10 parts of acrylate copolymer, 1-3 parts of surfactant, 0.2-0.6 part of additive, 0.1-0.6 part of anticorrosive agent and 8-40 parts of ultrapure water; the preparation method of the PI film stripping liquid comprises the following steps: placing grinding balls or stirring rods with different sizes into a container with a stirring function, then injecting ultrapure water into the container, sequentially adding an acrylate copolymer, a surfactant, an additive and an anticorrosive agent under the stirring condition, and stirring for 20-40 min; slowly dripping aqueous organic solvent and organic amine under the condition of stirring, uniformly stirring, heating to 100-120 ℃, concentrating to two thirds of the total volume, and filtering to obtain PI membrane stripping liquid. The invention overcomes the defects of the prior art, reduces the content of impurity metal ions and particles in the PI film stripping solution, improves the permeability and improves the stripping effect of the stripping solution.
Description
Technical Field
The invention relates to the technical field of stripping liquid, and particularly belongs to PI film stripping liquid.
Background
The PI liquid (the main component is polyimide) is an essential substance in the production process of the thin film transistor liquid crystal display, and the PI liquid is coated on glass and baked to form a PI film. After the PI film is rubbed or illuminated, the PI film has an alignment effect on the liquid crystal material, so that the consistency of the rotation direction of liquid crystal molecules is better, the liquid crystal deflects under the action of an electric field, and the PI film has a switching effect on an optical path.
In the production process of the PI film process, the yield of one-time coating is not high, and in order to reduce the loss of raw materials, a certain technology is required to remove the PI film, so that the glass substrate is recycled. In addition, it is common to check whether the coating is uniform, using a debugging glass, which is initially printed for checking the print quality. In order to save cost, the PI film on the surface of the polyimide film can be removed and used repeatedly.
Currently, the dry method PI film removal process is used below the G8.5 generation line, and the specific process is to decompose the PI film by plasma oxidation. However, for more than G8.5 generation, there is no corresponding dry equipment, and only the PI film can be removed by a wet process technique, and the PI film is removed by the stripping ability of the stripping liquid, so that the glass substrate can be reused.
The PI film stripping liquid can quickly dissolve the PI film, cannot corrode an integrated circuit and a related organic film layer below the PI film, and can simultaneously take stripping effects of various PI films into consideration. In addition, the content of the particles in the PI film stripping liquid is controlled within a certain range. The technology has high threshold and great difficulty, the current products are mainly from Japanese and Korean manufacturers, and the related products of the PI film stripping liquid are not developed in China. Therefore, the realization of the localization of the technology is a difficult problem which needs to be solved urgently. The invention develops one or a series of low-temperature water systems, low-particulate-matter-content and environment-friendly PI stripping solutions, can efficiently remove PI films, and fills the domestic technical blank.
Disclosure of Invention
The invention aims to provide a PI film stripping liquid, overcomes the defects of the prior art, reduces the particulate content of the PI film stripping liquid, improves the permeability, improves the stripping effect of the stripping liquid, and does not corrode a bottom glass substrate.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the PI film stripping liquid comprises the following raw materials in parts by weight:
12-35 parts of water-soluble organic solvent, 3-15 parts of organic amine, 2-10 parts of acrylate copolymer, 1-3 parts of surfactant, 0.2-0.6 part of additive, 0.1-0.6 part of anticorrosive agent and 8-40 parts of ultrapure water;
the preparation method of the PI film stripping liquid comprises the following steps:
(1) weighing the raw materials according to the parts by weight;
(2) placing grinding balls or stirring rods with different sizes into a container with a stirring function, then injecting ultrapure water into the container, sequentially adding an acrylate copolymer, a surfactant, an additive and an anticorrosive agent under the stirring condition, and stirring for 20-40 min;
(3) slowly dripping aqueous organic solvent and organic amine into the system in the step (2) under the condition of stirring, uniformly stirring, heating to 100 ℃ and 120 ℃, concentrating to two thirds of the total volume, and filtering to obtain PI membrane stripping liquid.
Further, the water-soluble organic solvent comprises a composition of two or more of propylene glycol monomethyl ether, propylene glycol ethyl ether, propylene glycol monomethyl ether acetate, butyl methacrylate, cyclohexane, cyclohexanone, butyl carbitol, 3-ethyl propionate, butyl carbitol acetate and gamma-butyrolactone.
Further, the organic amine is selected from any one or a mixture of any more of diethylamine, triethylamine, ethylenediamine, monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine and triisopropanolamine.
Further, the surfactant is polyoxyethylene ether or polyoxypropylene ether.
Further, the additive includes an azole compound.
Further, the anticorrosive agent adopts phytate.
Further, the stirring speed in the step (2) and the step (3) is 500r/min, the stirring is stopped and the mixture is kept stand for 1-3min during the stirring process, the stirring is started rapidly, and the circulation is repeated for 2-3 times by controlling each component to be added.
Further, the filtering in the step (3) comprises coarse filtering and fine filtering, wherein the coarse filtering adopts a filter screen with the aperture of 0.1-0.3mm, the fine filtering adopts a filter screen with the aperture of 0.1-0.5um, the fine filtering is repeated for 2-3 times, and in addition, the deionized filtering is included.
Further, the technical specification of the obtained PI film stripping solution is as follows: the content of impurity metal ions in the PI film stripping liquid is less than or equal to 90ppb, and the content of particles (more than or equal to 0.5 mu m) is less than or equal to 50/mL.
The invention also provides a PI film stripping method, which adopts any one of the PI film stripping liquids.
Further, the method specifically comprises the following steps:
(1) soaking the glass substrate with the PI film in PI film stripping liquid at 20-60 ℃ for 1-60 minutes;
(2) rinsing the glass substrate after the PI film is removed for 3-10 minutes by using pure water, rinsing for 1-3 times, and then drying by using nitrogen.
Compared with the prior art, the invention has the following implementation effects:
according to the PI film stripping liquid, the solubility and the stripping property of the stripping liquid are improved by adding the acrylate copolymer and the surfactant; by improving the preparation method, the content of particles in the stripping liquid is lower, the stripping liquid is finer and smoother, the permeability is better, and the stripping property of the stripping liquid is further improved.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples, and any modification is within the scope of the present invention without departing from the spirit of the present invention.
Example 1
The embodiment discloses a PI film stripping liquid which comprises the following raw materials in parts by weight:
12 parts of water-soluble organic solvent, 3 parts of organic amine, 2 parts of acrylate copolymer, 1 part of surfactant, 0.2 part of additive, 0.1 part of anticorrosive and 8 parts of ultrapure water;
the preparation method of the PI film stripping liquid comprises the following steps:
(1) weighing the raw materials according to the parts by weight;
(2) placing grinding balls or stirring rods with different sizes into a container with a stirring function, then injecting ultrapure water into the container, sequentially adding an acrylate copolymer, a surfactant, an additive and an anticorrosive agent under the stirring condition, and stirring for 20-40 min;
slowly dripping aqueous organic solvent and organic amine into the system in the step (2) under the condition of stirring, uniformly stirring, heating to 100 ℃ and 120 ℃, concentrating to two thirds of the total volume, and filtering to obtain PI membrane stripping liquid.
Further, the water-soluble organic solvent comprises a combination of two or more of propylene glycol monomethyl ether, propylene glycol ethyl ether, propylene glycol monomethyl ether acetate, butyl methacrylate, cyclohexane, cyclohexanone, butyl carbitol, 3-ethyl propionate, butyl carbitol acetate and gamma-butyrolactone.
Further, the organic amine is selected from any one or a mixture of any more of diethylamine, triethylamine, ethylenediamine, monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine.
Further, the surfactant is polyoxyethylene ether or polyoxypropylene ether.
Further, the additive includes an azole compound.
Further, the anticorrosive agent employs phytate.
Further, the stirring speed in the step (2) and the step (3) is 500r/min, the stirring is stopped and the mixture is kept stand for 1-3min during the stirring process, the stirring is started rapidly, and the circulation is repeated for 2-3 times by controlling each component to be added.
Further, the filtering in step (3) comprises coarse filtering and fine filtering, wherein the coarse filtering adopts a filter screen with the aperture of 0.1-0.3mm, the fine filtering adopts a filter screen with the aperture of 0.1-0.5um, the fine filtering is repeated for 2-3 times, and additionally, deionized filtering is included.
Further, the technical specification of the obtained PI film stripping solution is as follows: the content of impurity metal ions in the PI film stripping liquid is less than or equal to 90ppb, and the content of particles (more than or equal to 0.5 mu m) is less than or equal to 50/mL.
Example 2
The raw material ratio and the preparation method of the PI film stripping solution disclosed in this example are substantially the same as those of example 1, except that: the raw material proportion of the PI film comprises 23 parts of water-soluble organic solvent, 9 parts of organic amine, 6 parts of acrylate copolymer, 2 parts of surfactant, 0.4 part of additive, 0.35 part of anticorrosive agent and 19 parts of ultrapure water.
Example 3
The raw material ratio and the preparation method of the PI film stripping solution disclosed in this example are substantially the same as those of example 1, except that: the raw material proportion of the PI film comprises 30 parts of water-soluble organic solvent, 15 parts of organic amine, 10 parts of acrylate copolymer, 3 parts of surfactant, 0.6 part of additive, 0.6 part of anticorrosive agent and 30 parts of ultrapure water.
Comparative example 1
The proportion of the raw materials and the preparation method of the PI film stripping liquid disclosed by the comparative example are basically the same as those of the example 1, except that: no acrylic copolymer was added.
Comparative example 2
The proportion of the raw materials and the preparation method of the PI film stripping liquid disclosed by the comparative example are basically the same as those of the example 1, except that: no grinding balls or stirring rods are added in the stirring process.
And (3) performance detection:
the method for evaluating the PI removal ability of the stripping solution comprises the following steps: the glass substrate coated with the PI film of 100nm thickness was immersed in the PI film-peeling solutions produced in examples 1 to 3 and comparative examples 1 to 2 at 40 ℃ for 3 minutes, and the glass substrate after removal of the PI film was rinsed with pure water for 3 to 10 minutes, 1 to 3 times, and then dried with nitrogen. The specific PI film removing effect method is to visually determine whether the PI film is remained under a strong light, observe whether the PI film is remained and the corrosion condition by a 5-100 multiplied microscope, and measure the film thickness data. Specific results are shown in table 1.
TABLE 1 statistical Table of peeling effects of PI film peeling liquids
According to the statistical results in table 1, the PI film stripping solution provided by the invention has good permeability and stripping effect, not only can quickly remove the PI film on the surface of the substrate, but also can be completely and cleanly removed without corroding metal wiring, thereby being beneficial to subsequent production and improving the yield of products.
The foregoing is merely exemplary and illustrative of the present inventive concept and various modifications, additions and substitutions of similar embodiments may be made to the specific embodiments described by those skilled in the art without departing from the inventive concept or exceeding the scope of the claims as defined in the accompanying claims.
Claims (10)
1. A PI film stripping liquid is characterized in that: the composite material comprises the following raw materials in parts by weight:
12-35 parts of water-soluble organic solvent, 3-15 parts of organic amine, 2-10 parts of acrylate copolymer, 1-3 parts of surfactant, 0.2-0.6 part of additive, 0.1-0.6 part of anticorrosive agent and 8-40 parts of ultrapure water;
the preparation method of the PI film stripping liquid comprises the following steps:
(1) weighing the raw materials according to the parts by weight;
(2) placing grinding balls or stirring rods with different sizes into a container with a stirring function, then injecting ultrapure water into the container, sequentially adding an acrylate copolymer, a surfactant, an additive and an anticorrosive agent under the stirring condition, and stirring for 20-40 min;
(3) slowly dripping aqueous organic solvent and organic amine into the system in the step (2) under the condition of stirring, uniformly stirring, heating to 100 ℃ and 120 ℃, concentrating to two thirds of the total volume, and filtering to obtain PI membrane stripping liquid.
2. The PI film stripping solution according to claim 1, wherein: the water-soluble organic solvent comprises two or more of propylene glycol monomethyl ether, propylene glycol ethyl ether, propylene glycol monomethyl ether acetate, butyl methacrylate, cyclohexane, cyclohexanone, butyl carbitol, 3-ethyl ether propionate, butyl carbitol acetate and gamma-butyrolactone.
3. The PI film stripping solution according to claim 1, wherein: the organic amine is selected from any one or a mixture of any more of diethylamine, triethylamine, ethylenediamine, monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine and triisopropanolamine.
4. The PI film stripping solution according to claim 1, wherein: the surfactant is polyoxyethylene ether or polyoxypropylene ether.
5. The PI film stripping solution according to claim 1, wherein: the additive includes an azole compound.
6. The PI film stripping solution according to claim 1, wherein: the anticorrosive agent adopts phytate.
7. The PI film stripping solution according to claim 1, wherein: the stirring speed in the step (2) and the step (3) is 500r/min, the stirring is stopped and the mixture stands for 1 to 3min in the stirring process, the stirring is quickly started, and the circulation is controlled to be repeated for 2 to 3 times when each component is added.
8. The PI film stripping solution according to claim 1, wherein: the filtration in step (3) comprises coarse filtration and fine filtration, wherein the coarse filtration adopts a filter screen with pore size of 0.1-0.3mm, and the fine filtration adopts a filter screen with pore size of 0.1-0.5 μm, wherein the fine filtration is repeated for 2-3 times, and additionally comprises deionization filtration.
9. The PI film stripping solution as claimed in claims 1 to 8, which has the technical specifications that: the content of impurity metal ions in the PI film stripping liquid is less than or equal to 90ppb, and the content of particles (more than or equal to 0.5 mu m) is less than or equal to 50/mL.
10. The method for peeling a PI film according to claim 9, wherein: the method specifically comprises the following steps:
(1) soaking the glass substrate with the PI film in PI film stripping liquid at 20-60 ℃ for 1-60 minutes;
(2) rinsing the glass substrate after the PI film is removed for 3-10 minutes by using pure water, rinsing for 1-3 times, and then drying by using nitrogen.
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CN202011334406.5A CN112230520A (en) | 2020-11-24 | 2020-11-24 | Water-based PI film stripping liquid and PI film glass method thereof |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2008081045A1 (en) * | 2007-01-05 | 2008-07-10 | Basf Se | Composition and method for stripping organic coatings |
CN102147576A (en) * | 2010-02-09 | 2011-08-10 | 京东方科技集团股份有限公司 | Photoresist stripping liquid composite |
CN107102517A (en) * | 2017-06-02 | 2017-08-29 | 合肥市惠科精密模具有限公司 | A kind of AMOLEED display screens remover composition with photoresist |
CN110727181A (en) * | 2019-08-09 | 2020-01-24 | 华璞微电子科技(宁波)有限公司 | Positive photoresist stripping liquid composition |
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2020
- 2020-11-24 CN CN202011334406.5A patent/CN112230520A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008081045A1 (en) * | 2007-01-05 | 2008-07-10 | Basf Se | Composition and method for stripping organic coatings |
CN102147576A (en) * | 2010-02-09 | 2011-08-10 | 京东方科技集团股份有限公司 | Photoresist stripping liquid composite |
CN107102517A (en) * | 2017-06-02 | 2017-08-29 | 合肥市惠科精密模具有限公司 | A kind of AMOLEED display screens remover composition with photoresist |
CN110727181A (en) * | 2019-08-09 | 2020-01-24 | 华璞微电子科技(宁波)有限公司 | Positive photoresist stripping liquid composition |
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